1、Designation:D317507 Designation: D3175 11Standard Test Method forVolatile Matter in the Analysis Sample of Coal and Coke1This standard is issued under the fixed designation D3175; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method determines
3、the percentage of gaseous products, exclusive of moisture vapor, in the analysis sample whichare released under the specific conditions of the test.1.2 This test method for determination of volatile matter is empirical; because of its empirical nature, strict adherence to basicprincipals and permiss
4、ible procedures is required to obtain valid results.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of
5、regulatorylimitations prior to use.1.4 The values stated in SI units are to be regarded as the standard.2. Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of Coke Samples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Meth
6、od for Moisture in the Analysis Sample of Coal and Coke3. Terminology3.1 Definition:3.1.1 sparking fuelswithin the context of this test method, fuels that do not yield a coherent cake as residue in the volatilematter determination but do evolve gaseous products at a rate sufficient to mechanically c
7、arry solid particles out of the cruciblewhen heated at the standard rate. Such coals normally include all low-rank noncaking coals and lignites but can also include thoseanthracites, semianthracites, bituminous, and cokes that lose solid particles as described above. These are defined as sparking fu
8、elsbecause particles escaping at the higher temperatures can become incandescent and spark as they are emitted.4. Summary of Test Method4.1 Volatile matter is determined by establishing the loss in weight resulting from heating a coal or coke under rigidly controlledconditions. The measured weight l
9、oss, corrected for moisture as determined in Test Method D3173 establishes the volatile mattercontent. Two procedures are described to permit conformity with differences in sample behavior.4.2 In this empirical test method, the use of platinum crucibles shall be considered the standard reference met
10、hod for volatilematter. Platinum crucibles shall be used in determining the volatile matter of coke and volatile matter determined for classificationof coals by rank. Volatile matter determinations by some laboratories using alternate nickel-chromium alloy crucibles having thephysical dimensions spe
11、cified in 6.1 have been shown to differ from those obtained using platinum crucibles.Alaboratory utilizingnickel-chromium crucibles shall first determine if a relative bias exists between the use of nickel-chromium and platinum crucibleson the coals being tested using the test method set forth in An
12、nex A. Where a relative bias is shown to exist, the volatile matterdetermined using nickel-chromium crucibles shall be corrected by a factor determined through comparison of volatile matterresults from both crucible types on coals being tested or analysis of samples of known proximate analysis.5. Si
13、gnificance and Use5.1 Volatile matter, when determined as herein described, can be used to establish the rank of coals, to indicate coke yield on1This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of An
14、alysis.Current edition approved MarchApril 1, 2007.2011. PublishedApril 2007.2011. Originally approved in 1973. Last previous edition approved in 20022007 as D3175 027.DOI: 10.1520/D3175-07.10.1520/D3175-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Custome
15、r Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the
16、previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright AST
17、M International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.carbonization process, to provide the basis for purchasing and selling, or to establish burning characteristics.6. Apparatus6.1 Platinum Crucible, with closely fitting cover, for coal. The crucible s
18、hall be of not less than 10 or more than 20-mL capacity,not less than 25 or more than 35 mm in diameter, and not less than 30 or more than 35 mm in height.6.2 Platinum Crucible, with closely fitting cover, for coke. The crucible shall be of 10-mL capacity, with capsule cover havingthin flexible side
19、s fitting down into crucible. Or the double-crucible method can be used, in which the sample is placed in 10-mLplatinum crucible, which is then covered with another crucible of such a size that it will fit closely to the sides of the outer crucibleand its bottom will rest 8.5 to 12.7 mm (13 to12 in.
20、) above the bottom of the outer crucible.6.3 Alternate Crucible Materials, Nickel-chromium crucible with closely fitting cover. The crucible shall not be less than 10or more than 20 mL capacity, not less than 25 or more than 35 mm in diameter, and not less than 30 or more than 35 mm in height.Nickel
21、-chromium crucibles shall be heat-treated for4hat500C to ensure that they are completely oxidized prior to use.6.4 Vertical Electric Tube Furnace, for coal or coke. The electric furnace shall be a vertical tube furnace. The furnace can beof the form shown in Fig. 1. It shall be regulated to maintain
22、 a temperature of 950 6 20C in the crucible, as measured by athermocouple positioned in the furnace. The furnace shall accommodate sparking coals and meet the specifications set forth in7.3.2.6.5 Balance, sensitive to 0.1 mg.7. Procedure7.1 The sample shall be the material pulverized to No. 60 (250-
23、m) sieve in accordance with Practice D2013 or Practice D346.7.2 Procedure for Nonsparking Coals and Cokes:7.2.1 Weigh1gofthesample in a weighed platinum crucible, close with a cover which fits closely enough so that the carbondeposit from bituminous, subbituminous, and lignite coals does not burn aw
24、ay from the underside, place on platinum orNichrome-wire supports and insert directly into the furnace chamber, which shall be maintained at a temperature of 950 6 20C,and lower immediately to the 950C zone. Regulation of the temperature to within the prescribed limits is critical. After the morerap
25、id discharge of volatile matter has subsided, as shown by the disappearance of the luminous flame, or in the case of coke, after2 or 3 min, inspect the crucible (see Note 1) to verify that the lid is still properly sealed. If necessary, reseat the lid to guard againstthe admission of air into the cr
26、ucible. Do this as rapidly as possible by raising the crucible to the top of the furnace chamber,reposition the lid to more perfectly seal the crucible, then lower the crucible immediately back to the 950C zone. After heatingfor a total of exactly 7 min, remove the crucible from the furnace and with
27、out disturbing the cover, allow it to cool. Coke shouldbe cooled in a desiccator. Weigh as soon as cold. The percentage loss of weight minus the percentage moisture equals the volatilematter. With some strongly caking low-volatile and medium-volatile bituminous coals, the coke button can be broken w
28、ithexplosive violence due to the liberation of volatile matter within the button. This is usually designated as popping. Such poppingcan blow the lid off the crucible and cause mechanical losses of the coked material. When such popping is observed, thedetermination shall be rejected and the test rep
29、eated until popping does not occur.NOTE 1Inspection of the crucible can be aided by the use of a mirror held above the furnace well.7.3 Modified Procedure for All Sparking Fuels:7.3.1 Fuels that do not cake or cake weakly when volatile matter is determined shall be watched closely for sparking durin
30、gthe heating period (see Note 2); also, at the end of the test the crucible cover shall be inspected for ash deposits, and the presenceof such deposits shall be considered as evidence of sparking.7.3.2 All fuels that spark when the volatile matter is determined by the methods described in 7.1 shall
31、be treated as follows:The sample shall be given a preliminary gradual heating such that a temperature of 600 6 50C is reached in 6 min (Note 2). Afterthis preliminary heating the sample shall be heated for exactly 6 min at 950 6 20C. If sparking is then observed, the determinationshall be rejected a
32、nd the test repeated until no sparking occurs either during the preliminary heating or during the 6-min periodat 950C. Remove the crucible from the furnace, cool on a metal cooling block, and weigh. To ensure uniformity of results, keepthe cooling period constant and do not prolong beyond 15 min. Th
33、e percentage loss in weight minus the percent moisture inaccordance with Test Method D3173, is the volatile matter. All analyses by this test method shall be so marked when reported toindicate that the modified procedure was used.NOTE 2If a tubular furnace of the Fieldner type (Fig. 1) is used for t
34、he determination of volatile matter, the preliminary gradual heating can beaccomplished by moving the crucible to predetermined positions in the cooler top zone of the furnace. Due to variations in the heating characteristicsof the furnace, the operator shall predetermine by thermocouple the proper
35、positions to meet a preliminary heating rate as specified in 7.3.2. A mechanicaldevice to lower the crucible into the furnace can be used to facilitate control of the lowering operation.8. Calculation8.1 Calculate the weight loss percent as follows:Weight loss, % 5 A 2 B!/A 3 100 (1)D3175 112where:A
36、 = weight of sample used, g, andB = weight of sample after heating, g.8.2 Calculate the volatile matter percent in the analysis samples as follows:Volatile matter in analysis sample , % 5 C 2 D (2)where:C = weight loss, %, andD = moisture, %.9. Precision and Bias9.1 The precision of this test method
37、 for the determnination of Volatile Matter in Coal are shown in Table 1. Coal RepeatabilityFIG. 1 Electric Furnace for Determining Volatile MatterD3175 113and Reproducibility limits for this test method were determined using only platinum crucibles. Coal Repeatability andReproducibility limits for n
38、ickel-chromium crucibles have not been determined.9.1.1 Repeatability Limit (r)The value below which the absolute difference between two test results of separate andconsecutive test determinations, carried out on the same sample, in the same laboratory, by the same operator, using the sameapparatus
39、on samples taken at random from a single quantity of homogeneous material, can be expected to occur with a probabilityof approximately 95 %.9.1.2 Reproducibility Limit (R)The value below which the absolute difference between two test results carried out in differentlaboratories, using samples taken
40、at random from a single quantity of material that is as homogeneous as possible, can be expectedto occur with a probability of approximately 95 %.9.29.2 The precision of this test method for the determination of Volatile Matter in Coke are shown in Table 2. The precisioncharacterized by repeatabilit
41、y (Sr, r) and reproducibility (SR, R) is described in Table Table A2.1 in Annex A2.9.3 BiasSince this is an empirical test method when utilizing platinum crucibles, the degree of absolute bias can not bedetermined. Bias between the use of platinum and nickel-chromium crucibles shall be determined in
42、 the laboratory on coal beingtested using the test method set forth in Annex A.ANNEXANNEXESA1. METHOD FOR DETERMINING RELATIVE BIAS BETWEEN PLATINUM AND NICKEL-CHROMIUM ALLOYCRUCIBLESA1.1 ScopeA1.1.1 This method describes the procedure for determining the component of relative bias between platinum
43、and alternatenickel-chromium alloy crucibles.A1.2 ApparatusA1.2.1 All Apparatus and equipment shall conform to the apparatus and equipment specifications given in the “Apparatus”Section of Test Method D3175 with the additional requirement that temperatures shall be measured with a Type K or Nthermoc
44、ouple with a standard tolerance of 6 2.2 C.A1.3 ProcedureA1.3.1 Apply one of the two alternate methods given in the “Procedure” section of ASTM D3175 to a minimum of twenty pairsof the materials being tested, one member of each pair consisting of a one-gram analysis sample in a platinum crucible, an
45、d theTABLE 1 Concentrations Range andLimits for Repeatability andReproducibility of Volatile Matter in CoalRank, % RepeatabilityLimit,rReproducibilityLimit,RRank RepeatabilityLimit,rReproducibilityLimit,RHigh-temperature coke 0.2 0.4Anthracite 0.3 0.6Semianthracite, bituminous,low-temperature coke 0
46、.5 1.0Subbituminous 0.7 1.4Lignite 1.0 2.0TABLE 2 Concentration Range and Limits for Repeatability andReproducibility of Volatile Matter in CokeRange RepeatabilityLimit,rReproducibilityLimit,RCoke 0.49 to 2.50 % 0.20 0.27 + 0.27xAAWhere x is the average of two single test results.D3175 114other memb
47、er of each pair consisting of a one-gram analysis sample of the same material in a nickel-chromium alloy crucible.A1.3.2 The following additional limitations apply:A1.3.2.1 The materials in the study group shall all be of the same groupings listed in Table 1:1. Anthracite2. Semianthracite, Bituminou
48、s3. Subbituminous4. LigniteA1.3.2.2 The range of volatile matter contents within the study group shall not exceed 10% absolute. If the range of volatilematter routinely analyzed and within the same Table 1 grouping exceeds 10% absolute, analyze multiple groups to accommodatethe expected range of vol
49、atile matter. Apply the appropriate relative bias to samples within the same volatile matter range. Therelative bias shall be applicable only to analyses performed in the laboratory in which it is originally determined.A1.3.2.3 All values determined in any experiment upon members of the study group shall be used in the statistical analysis(unless there is undeniable evidence that the data to be rejected is technically invalid).A1.3.2.4 All materials within the study group shall be analyzed the same number of times.A1.3.2.5 Confirmatory analyses for each stu
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